EP3069376B1 - Verfahren zur isolierung von ionen - Google Patents

Verfahren zur isolierung von ionen

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Publication number
EP3069376B1
EP3069376B1 EP14796879.6A EP14796879A EP3069376B1 EP 3069376 B1 EP3069376 B1 EP 3069376B1 EP 14796879 A EP14796879 A EP 14796879A EP 3069376 B1 EP3069376 B1 EP 3069376B1
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EP
European Patent Office
Prior art keywords
ions
mass
ion
chemical compounds
derived
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EP14796879.6A
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English (en)
French (fr)
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EP3069376A2 (de
Inventor
John Brian Hoyes
Steven Derek Pringle
Farnoush SALARZAEI
Jason Lee Wildgoose
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Micromass UK Ltd
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Micromass UK Ltd
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Priority claimed from GBGB1319952.6A external-priority patent/GB201319952D0/en
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Priority to EP14796879.6A priority Critical patent/EP3069376B1/de
Publication of EP3069376A2 publication Critical patent/EP3069376A2/de
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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622—Ion mobility spectrometry
    • G01N27/623—Ion mobility spectrometry combined with mass spectrometry
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0027—Methods for using particle spectrometers
    • H01J49/0031—Step by step routines describing the use of the apparatus
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/40—Time-of-flight spectrometers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/42—Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
    • H01J49/4205—Device types
    • H01J49/421—Mass filters, i.e. deviating unwanted ions without trapping
    • H01J49/4215—Quadrupole mass filters

Definitions

  • mass spectrometry for separating one type of ion from other ions prior to analysis.
  • a mass filter may be used to mass selectively transmit only one type of ion in order to isolate a desired type of ion.
  • an ion mobility separator may be used to separate ions from each other according to their ion mobilities.
  • the present invention provides a method of mass spectrometry as claimed in claim 1.
  • the present invention provides a convenient and efficient method of isolating a group of different ions derived from chemical compounds in the same class. Other ions are removed, rendering detection and mass analysis of said different ions particularly efficient.
  • the mass filter is varied with time such that ions derived from different chemical compounds that are in the same chemical class are preferably substantially isolated from all other ions. Ions not from said chemical class are not transmitted.
  • EP 1365438 It is known to selectively transmit ions having desired combinations of ion mobility and mass to charge ratio for the purpose of charge state selection, for example, from EP 1365438 .
  • EP 1365438 does not recognise that compounds in the same chemical class have ion mobilities and mass to charge ratios that follow a relationship. As such, this document does not disclose or suggest the concept of isolating a group of different ions derived from chemical compounds in the same class.
  • US 2002/014586 discloses in general the features of separating ions by ion mobility and mass filtering ions. However, this document also does not disclose or suggest the concept of isolating a group of different ions derived from chemical compounds in the same class.
  • MICHAL KLIMAN ET AL "Lipid analysis and lipidomics by structurally selective ion mobility-mass spectrometry", BIOCHIMICA ET BIOPHYSICA ACTA (BBA) - MOLECULAR AND CELL BIOLOGY OF LIPIDS, ELSEVIER, AMSTERDAM, NL, vol. 1811, no. 11, 23 May 2011 (2011-05-23), pages 935-945, 1388-1981, DOI: 10.1016/J.BBALIP.2011.05.016 also discloses the features of separating ions by ion mobility and mass filtering ions. Separate mass spectra are generated for ions generated from different classes of substances. However these are derived from data analysis of the two dimensional spectra.
  • ions derived from chemical compounds in the same class is preferably intended to mean ionised chemical compounds in the same class. Said different ions are preferably produced by ionising an analyte and are not fragment ions.
  • the group of different ions is a group of different types of ions.
  • the class of chemical compounds preferably corresponds to compounds that share one or more common functional group or share a common moiety such that the one or more functional group or moiety provides the compounds with similar chemical reactivity or with a common chemical property.
  • the compounds in said class of compounds have a common functional group or moiety that defines said class of compounds.
  • each of said different ions includes said one or more functional group or said moiety.
  • Said class of compounds is preferably one of: lipids, pesticides; metabolites; peptides; proteins; antibodies; enzymes; a class of compounds with related biological function or activity; a class of compounds with related chemical structure; a class of compounds with related chemical reactivity; or a class of compounds with related solution chemistry.
  • substantially only ions derived from said chemical compounds in the same class of compounds are transmitted by the mass filter and all other ions are not transmitted by the mass filter and are rejected.
  • Said other ions may be background matrix ions that have the same charge state as at least some of the ions derived from chemical compounds in the same class. At least some of said ions derived from chemical compounds in the same class are preferably singly charged ions and/or said other ions are preferably singly charged ions.
  • said different ions derived from chemical compounds in the same class consist of or comprise singly charged ions and said other ions also consist of or comprise singly charged ions.
  • the mass to charge ratios of said different ions vary as a function of their ion mobilities such that the ions from the same class of chemical compounds follow a trend; and wherein the mass to charge ratios transmitted by the mass filter vary with time so as to follow said trend and thereby transmit the ions from the same class of chemical compound and filter out other ions.
  • the relationship between the mass to charge ratios and the ion mobilities of said different ions may be such that the mass to charge ratios of the ions increase substantially continuously with increasing ion mobility.
  • the mass to charge ratios of said different ions derived from chemical compounds in the same class may vary as a substantially linear or polynomial function of their ion mobility.
  • the mass filter may be operated so as to only transmit ions having a mass to charge ratio greater than a minimum value and a mass to charge ratio less than a maximum value, and the mass filter may be is scanned with time so that said minimum value and said maximum value are progressively increased with time.
  • the mass filter may be scanned in a continuous or in a stepped manner.
  • the different ions are mass analysed after they have been transmitted by the mass filter.
  • the mass analyser may comprise a detector that detects the ions.
  • the temporal separation of the different ions is preferably removed by transmitting the separated and mass filtered ions into a region comprising a collisional gas such that the ions collide with the gas and said different ions intermix.
  • the preferred embodiment counteracts the loss in dynamic range of the instrument that would otherwise be associated with the temporal compression or concentration of the ion populations introduced by the ion mobility separator. This is a particular issue when a time of Flight (ToF) mass analyser is arranged downstream of the mass filter, as the dynamic range of the instrument is already restricted by the detection system of the ToF mass analyser. Accordingly, the mass analyser used in the present invention may be a ToF mass analyser. Removing the temporal separation also removes the data storage requirements of the instrument as the ion mobility data is no longer stored.
  • ToF time of Flight
  • a Time of Flight mass analyser is preferred and the present invention may be employed in combination with other established Time of Flight enhancements such as EDC/HDC.
  • types of mass analyser other than a Time of Flight mass analyser may be used in the present invention.
  • an analytical quadrupole mass analyser with ion detector may replace the Time of Flight mass analyser in an IMS-Q-Q arrangement.
  • Ions may be pulsed into the ion mobility separator a plurality of times.
  • a first pulse of ions may be pulsed into the ion mobility separator and the ions separated therein and a second pulse of ions may be subsequently pulsed into the ion mobility separator and the ions separated therein.
  • the mass to charge ratios of the ions transmitted by the mass filter may vary as a function of ion mobility separator drift time according to a first function for the ions from the first ion pulse, and may vary as a second different function for the ions from the second pulse.
  • Third or further pulses of ions may be provided and the mass filter may vary according to a third or further function respectively.
  • the precursor ions are separated by ion mobility separation through a gas
  • the ions may alternatively be separated according to Field Asymmetric Ion Mobility Separation (FAIMS), or according to a physicochemical property other than ion mobility or FAIMS.
  • FIMS Field Asymmetric Ion Mobility Separation
  • the method may be operated in a first mode so that at least some of the ions transmitted by the mass filter are fragmented or reacted so as to produce fragment or product ions, and said step of mass analysing may comprise mass analysing the fragment or product ions.
  • the method may also be operated in a second mode so that at least some of the ions transmitted by the mass filter are not fragmented or reacted, and said step of mass analysing comprises mass analysing the precursor ions transmitted by the mass filter.
  • the method preferably further comprises identifying a precursor ion from one or more fragment or product ion determined to be associated with the precursor ion.
  • the present invention also provides a mass spectrometer arranged and configured to perform any one of the methods described herein.
  • the present invention provides a mass spectrometer as claimed in claim 13.
  • the mass spectrometer may comprises a device arranged and adapted to supply an AC or RF voltage to the electrodes.
  • the AC or RF voltage preferably has an amplitude selected from the group consisting of: (i) ⁇ 50 V peak to peak; (ii) 50-100 V peak to peak; (iii) 100-150 V peak to peak; (iv) 150-200 V peak to peak; (v) 200-250 V peak to peak; (vi) 250-300 V peak to peak; (vii) 300-350 V peak to peak; (viii) 350-400 V peak to peak; (ix) 400-450 V peak to peak; (x) 450-500 V peak to peak; and (xi) > 500 V peak to peak.
  • the AC or RF voltage preferably has a frequency selected from the group consisting of: (i) ⁇ 100 kHz; (ii) 100-200 kHz; (iii) 200-300 kHz; (iv) 300-400 kHz; (v) 400-500 kHz; (vi) 0.5-1.0 MHz; (vii) 1.0-1.5 MHz; (viii) 1.5-2.0 MHz; (ix) 2.0-2.5 MHz; (x) 2.5-3.0 MHz; (xi) 3.0-3.5 MHz; (xii) 3.5-4.0 MHz; (xiii) 4.0-4.5 MHz; (xiv) 4.5-5.0 MHz; (xv) 5.0-5.5 MHz; (xvi) 5.5-6.0 MHz; (xvii) 6.0-6.5 MHz; (xviii) 6.5-7.0 MHz; (xix) 7.0-7.5 MHz; (xx) 7.5-8.0 MHz; (xxi) 8.0-8.5 MHz; (xxii) 8.5
  • Fig. 1 shows a schematic of a preferred embodiment of the present invention.
  • This embodiment comprises an ion source 2, an ion mobility separator (IMS) 4, a quadrupole mass filter 6, a collision cell 8 and a Time of Flight mass analyser 10.
  • IMS ion mobility separator
  • ions are generated by the ion source 2 and are directed into the IMS device 4. Ions having different mobilities pass through the gas in the IMS device 4 with different drift times and so the IMS device 4 causes the ions to separate according to their ion mobility through the IMS device 4.
  • the quadrupole mass filter 6 is arranged between the IMS device 4 and the collision cell 8 and only transmits ions having a restricted range of mass to charge ratios at any given time.
  • the mass to charge ratio transmission window of the quadrupole mass filter 6 is scanned with time whilst the ions emerge from the IMS device 4 such that the mass filter 6 mass selectively transmits ions from the IMS device 4 to the collision cell 8.
  • a second mode of operation is also contemplated in which the ions are fragmented in the collision cell 8, e.g. via collisionally induce dissociation.
  • the resulting fragment ions are analysed in the ToF mass analyser 10.
  • the fragmentation device 8 may be repeatedly alternated between the first mode in which no fragmentation takes place and the second mode, such as in an MS e experiment.
  • the ion signal profile for the precursor ions varies as a function of the drift time through the IMS device 4.
  • the ion signal profile for a fragment ion can be matched to the ion signal profile for the precursor ions. This enables a fragment ion to be associated with an IMS drift time of its related precursor ion.
  • the precursor ions may be induced to fragment in the fragmentation device 8 by accelerating the ions into the fragmentation device 8 with sufficient energy such that the ions interact with a gas in the fragmentation device 8 and fragment.
  • the precursor ions may be induced to oscillate within a collision gas arranged in the fragmentation device 8 such that the precursor ions fragment.
  • Precursor ions having different drift times through the ion mobility separator 4 may be subjected to different fragmentation energies so as to cause them to fragment.
  • precursor ions having a first IMS drift time may be accelerated into the fragmentation device 8 with a first energy or using a first acceleration voltage difference such that the ions fragment in the fragmentation device 8; and precursor ions having a second IMS drift time may be accelerated into the fragmentation device 8 with a second, different energy or using a second different acceleration voltage difference such that the ions fragment in the fragmentation device 8.
  • precursor ions having a first IMS drift time may be caused to oscillate into fragmentation by an oscillating electric field having a first frequency and/or amplitude
  • precursor ions having a second IMS drift time may be caused to oscillate into fragmentation by an oscillating electric field having a second frequency and/or amplitude.
  • Other methods of fragmentation are also contemplated. It is also contemplated that instead of fragmenting the ions, or in addition, the ions may be reacted with other molecules or ions so as to form product ions.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Molecular Biology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Claims (13)

  1. Verfahren zur Massenspektrometrie, umfassend:
    Bereitstellen einer Gruppe verschiedener Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, vermischt mit anderen Ionen, die nicht aus chemischen Verbindungen der gleichen Klasse stammen, wobei zumindest einige der anderen Ionen den gleichen Ladungszustand aufweisen wie zumindest einige der Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, wobei die Klasse chemischer Verbindungen Verbindungen entspricht, die eine oder mehrere gemeinsame funktionelle Gruppen oder einen gemeinsamen Rest aufweisen, und wobei die verschiedenen Ionen unterschiedliche Masse-Ladungs-Verhältnisse und lonenmobilitäten aufweisen; und
    Isolieren der Gruppe verschiedener Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, von den anderen Ionen, die nicht aus chemischen Verbindungen der gleichen Klasse stammen, durch:
    (i) Erhalten einer bekannten Beziehung oder Bestimmen einer Beziehung zwischen den Masse-Ladungs-Verhältnissen und den lonenmobilitäten der verschiedenen Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen;
    (ii) zeitliches Trennen der Ionen entsprechend ihrer lonenmobilität in einem lonenmobilitätsseparator; und dann
    (iii) Massenfiltern der resultierenden getrennten Ionen entsprechend dem Masse-Ladungs-Verhältnis mit einem Massenfilter, wobei die vom Massenfilter übertragenen Masse-Ladungs-Verhältnisse mit der Zeit als eine Funktion der lonenmobilität, die vom lonenmobilitätsseparator am Massenfilter empfangen wird, und nach der Beziehung variiert werden, so dass die verschiedenen Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, vom Massenfilter übertragen werden und die anderen Ionen, die nicht aus chemischen Verbindungen der gleichen Klasse stammen, nicht vom Massenfilter übertragen werden;
    wobei das Verfahren weiter ein Aufheben der zeitlichen Trennung von Ionen umfasst, nachdem diese getrennt und massengefiltert wurden, und dann eine Massenanalyse der Ionen oder der davon stammenden Ionen umfasst.
  2. Verfahren nach Anspruch 1, wobei die Klasse chemischer Verbindungen Verbindungen entspricht, die eine oder mehrere gemeinsame funktionelle Gruppen oder einen gemeinsamen Rest aufweisen, so dass die eine oder mehreren funktionellen Gruppen oder der Rest den Verbindungen eine ähnliche chemische Reaktivität oder eine gemeinsame chemische Eigenschaft verleihen.
  3. Verfahren nach einem vorstehenden Anspruch, wobei die Klasse von Verbindungen eine von Folgenden ist: Lipide, Pestizide; Metaboliten; Peptide; Proteine; Antikörper; Enzyme; eine Klasse von Verbindungen mit verwandter biologischer Funktion oder Aktivität; eine Klasse von Verbindungen mit verwandter chemischer Struktur; eine Klasse von Verbindungen mit verwandter chemischer Reaktivität; oder eine Klasse von Verbindungen mit verwandter Lösungschemie.
  4. Verfahren nach einem vorstehenden Anspruch, wobei im Wesentlichen nur Ionen, die aus den chemischen Verbindungen der gleichen Verbindungsklasse stammen, durch das Massenfilter übertragen werden und andere Ionen nicht durch das Massenfilter übertragen werden.
  5. Verfahren nach einem vorstehenden Anspruch, wobei die verschiedenen Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, aus einfach geladenen Ionen bestehen oder diese umfassen und die anderen Ionen ebenfalls aus einfach geladenen Ionen bestehen oder diese umfassen.
  6. Verfahren nach einem vorstehenden Anspruch, wobei die Beziehung zwischen den Masse-Ladungs-Verhältnissen und den lonenmobilitäten der verschiedenen Ionen derart ist, dass die Masse-Ladungs-Verhältnisse der Ionen mit zunehmender lonenmobilität im Wesentlichen kontinuierlich zunehmen, und/oder wobei die Masse-Ladungs-Verhältnisse der verschiedenen Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, im Wesentlichen als eine lineare oder polynomische Funktion ihrer lonenmobilität variieren.
  7. Verfahren nach einem vorstehenden Anspruch, wobei die zeitliche Trennung der verschiedenen Ionen aufgehoben wird, indem die getrennten und massengefilterten Ionen in einen Bereich übertragen werden, der ein Kollisionsgas umfasst, so dass die Ionen mit dem Gas kollidieren und sich die verschiedenen Ionen vermischen.
  8. Verfahren nach einem vorstehenden Anspruch, wobei der Schritt zur Massenanalyse mit einem Flugzeit-Massenanalysator durchgeführt wird.
  9. Verfahren nach einem vorstehenden Anspruch, wobei die Ionen vom Massenfilter zu einem Massenanalysator übertragen werden, um die Massenanalyse durchzuführen, ohne in einer Ionenfalle eingefangen zu werden.
  10. Verfahren nach einem vorstehenden Anspruch, wobei in einem ersten Betriebsmodus zumindest einige der vom Massenfilter übertragenen Ionen fragmentiert oder umgesetzt werden, um Fragment- oder Produktionen zu erzeugen, und der Schritt zur Massenanalyse eine Massenanalyse der Fragment- oder Produktionen umfasst.
  11. Verfahren nach Anspruch 10, wobei in einem zweiten Betriebsmodus zumindest einige der vom Massenfilter übertragenen Ionen nicht fragmentiert oder umgesetzt werden, und der Schritt zur Massenanalyse eine Massenanalyse der vom Massenfilter übertragenen Vorläuferionen umfasst, wobei bei dem Verfahren wiederholt zwischen dem ersten und dem zweiten Modus gewechselt wird, während die aus chemischen Verbindungen der gleichen Klasse stammenden Ionen im lonenmobilitätsseparator, und während diese Ionen aus dem lonenmobilitätsseparator eluieren, zeitlich getrennt werden, wobei die Fragment- oder Produktionen, die im ersten Modus einer Massenanalyse unterzogen und erkannt werden, den Elutionszeiten zugeordnet sind, zu denen ihre jeweiligen Vorläuferionen aus dem lonenmobilitätsseparator eluiert werden; wobei die im zweiten Modus massenanalysierten und detektierten Vorläuferionen ihren Elutionszeiten aus dem lonenmobilitätsseparator zugeordnet sind; und wobei die im ersten Modus detektierten Fragment- oder Produktionen ihren jeweiligen Vorläuferionen zugeordnet sind, die im zweiten Modus erkannt werden, indem die den Fragment- oder Produktionen zugeordneten Elutionszeiten mit den den Vorläuferionen zugeordneten Elutionszeiten abgeglichen werden.
  12. Verfahren nach Anspruch 11, weiter umfassend Identifizieren eines Vorläuferions aus einem oder mehreren Fragmenten oder Produktionen, die nachweislich mit dem Vorläuferion in Zusammenhang stehen.
  13. Massenspektrometer, umfassend:
    Mittel zum Bereitstellen einer Gruppe verschiedener Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, vermischt mit anderen Ionen, die nicht aus chemischen Verbindungen der gleichen Klasse stammen, wobei zumindest einige der anderen Ionen den gleichen Ladungszustand aufweisen wie zumindest einige der Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, wobei die Klasse chemischer Verbindungen Verbindungen entspricht, die eine oder mehrere gemeinsame funktionelle Gruppen oder einen gemeinsamen Rest aufweisen, und wobei die verschiedenen Ionen unterschiedliche Masse-Ladungs-Verhältnisse und lonenmobilitäten aufweisen; und
    Mittel zum Isolieren der Gruppe verschiedener Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, von den anderen Ionen, die nicht aus den chemischen Verbindungen der gleichen Klasse stammen, umfassend:
    (i) Speichermittel zum Speichern einer Beziehung zwischen den Masse-Ladungs-Verhältnissen und den lonenmobilitäten der verschiedenen Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen;
    (ii) einen lonenmobilitätsseparator zum zeitlichen Trennen der Ionen entsprechend ihrer lonenmobilität;
    (iii) einen dem lonenmobilitätsseparator nachgeschalteten Massenfilter zum Massenfiltern der getrennten Ionen nach dem Masse-Ladungs-Verhältnis; und
    (iv) eine Steuereinheit, die so angeordnet und konfiguriert ist, dass sie die vom Massenfilter übertragenen Masse-Ladungs-Verhältnisse mit der Zeit als eine Funktion der vom lonenmobilitätsseparator am Massenfilter empfangenen lonenmobilitäten und nach dieser Beziehung variiert, so dass die verschiedenen Ionen, die aus chemischen Verbindungen der gleichen Klasse stammen, vom Massenfilter übertragen werden und die anderen Ionen, die nicht aus chemischen Verbindungen der gleichen Klasse stammen, nicht vom Massenfilter übertragen werden; und
    wobei das Spektrometer weiter Mittel zum Aufheben der zeitlichen Trennung von Ionen umfasst, wobei diese Mittel dem Massenfilter nachgeschaltet sind; und
    einen Massenanalysator zur Massenanalyse von Ionen.
EP14796879.6A 2013-11-12 2014-11-11 Verfahren zur isolierung von ionen Active EP3069376B1 (de)

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Applications Claiming Priority (4)

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EP13192581 2013-11-12
GBGB1319952.6A GB201319952D0 (en) 2013-11-12 2013-11-12 Methods of isolating ions
PCT/GB2014/053333 WO2015071647A2 (en) 2013-11-12 2014-11-11 Method of isolating ions
EP14796879.6A EP3069376B1 (de) 2013-11-12 2014-11-11 Verfahren zur isolierung von ionen

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EP3069376B1 true EP3069376B1 (de) 2025-08-20

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